梳型聚合物的合成及降凝性能研究
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摘要
本文结合苏丹三七区原油高含蜡、高胶质沥青质和高凝固点的特点,根据原油降凝机理合成了五种不同种类的梳型聚合物,通过红外(IR)对结构进行了表征,并就不同因素对降凝效果的影响作了研究探讨,具体内容如下:
1.以壬基酚与甲醛为原料,合成了线形聚合物酚醛树脂,通过实验确定了最佳合成工艺条件,以醋酸锌为催化剂,调节反应PH值至4—7范围内,壬基酚与甲醛摩尔比1:1.5,反应温度85℃,反应时间4h。
2.研究不同因素对酯化产率的影响,确定了丙烯酸十八酯合成的最佳工艺,丙烯酸与十八醇摩尔比为1:1.5;对甲苯磺酸的质量分数为0.7wt%;对苯二酚的质量分数为0.4wt%;反应温度为120℃;反应时间为4h;携水剂按醇酸总质量的50%计。在此反应条件下,酯化产率可达93%以上。
3.以碳酸乙烯酯、1,3—丙烷磺内酯、马来酸酐、苯乙烯、丙烯酰胺、高级醇等为原料合成了酚醛树脂接枝碳酸乙烯酯(A)、酚醛树脂接枝1,3—丙烷磺内酯(B)、马来酸酐—丙烯酸十八酯二元共聚物(C)、马来酸酐—苯乙烯—丙烯酸十八酯三元共聚物(D)、马来酸酐—苯乙烯—丙烯酰胺酯化物(E)等五种梳型聚合物,分别考察了其对原油的降凝效果,发现A、B两种降凝剂降凝效果较差,仅为0～1℃。降凝剂E降凝效果最好,达到6.5℃。
4.研究了梳型聚合物的链段分布、亲油端链段、引发剂用量、聚合温度、聚合时间、降凝剂加入量、降凝剂处理温度等因素对原油降凝效果的影响。随着亲油链段的增长,降凝效果越来越好。随着引发剂加入量的增加,降凝效果越来越好,进一步增加,降凝效果开始变差。随着聚合温度的提高、聚合时间的延长,降凝效果越来越好,最后趋于稳定。
5.确定了C、D、E三种降凝剂的最佳合成工艺,马来酸酐:丙烯酸十八酯(mol)=1:3,引发剂用量0.5wt%,聚合温度105℃,聚合时间4h时,马来酸酐:苯乙烯:丙烯酸十八酯(mol)=2:1:6,引发剂用量0.7wt%,聚合温度100℃,聚合时间6h,马来酸酐:苯乙烯:丙烯酰胺(mol)=6:1:2,引发剂用量0.6wt%,聚合温度100℃,聚合时间7h。
In view of crude oils of Sudan 3/7 areas' character of high paraffin,high asphaltum,high solidification point and the mechanism of depressing pour point,a series of comb copolymer was synthesized and characterized by infrared(IR).Factors to influence pour point were also investigated.
The concrete content is as follows
1.Nonyl phenol and formaldehyde were used as a raw material to prepare linear polymer phenolics.Optimum technic conditions were obtained as follows:Zinc acetate as catalyst,PH= 4-7,T=85℃,t=4h,nonyl phenol versus formaldehyde =1:1.5(mol).
2.Factors to influence production rate of esterification were investigated.And optimum technic conditions were obtained as follows:acrylacid versus Octadecanol=1:1.5(mol);the content of toluene sulfonic acid is 0.7wt%;the content of hydroquinonequality is 0.4wt%;T=120℃;t= 4h.Under experimental conditions,the esterification production rate may reach above 93%.
3.A series of comb polymers was synthesized as follows:Phenolics-Ethylene carbonate graft copolymer(A),the Phenolicsstem—1,3-Propane sultone graft copolymer(B),Maleic anhydride -Octadecyl acrylate bipolymers(C),Maleic anhydride-Styrene-Octadecyl acrylate(D),Maleic anhydride-Styrene-Acrylamide ester(E).The efficiency of depressing pour point was also studied.Results showed that the efficiency of A,B to depress pour point was bad,only 0～1℃, E was the best,achieving 6.5℃.
4.The factors of comb polymer segment distribution,hydrophobic chain,the content of initiator, polymerization temperature,polymerization time,the content of PPD,and crude oil post-processing temperature to depress pour point were investigated.With the increases of hydrophobic chain,the efficiency of depressing pour point became better.With the increases of polymerization temperature and time,the efficiency of depressing pour point became better, finally tended to stable.
5.Optimum technics conditions for C,D and E were obtained as follows:Maleic anhydride: Octadecyl acrylate=1:3(mol),the content of initiator is 0.5wt%,T=105℃,t=4h for C;Maleic anhydride:Styrene:Octadecyl acrylate =2:1:6(mol),the content of initiator is 0.7wt%,T=100℃,t=6h for D;Maleic anhydride:Styrene:Acrylamide=6:1:2(mol),the content of initiator is 0.6wt%,T=100℃,t=8h.for E,repectively.
1.以壬基酚与甲醛为原料,合成了线形聚合物酚醛树脂,通过实验确定了最佳合成工艺条件,以醋酸锌为催化剂,调节反应PH值至4—7范围内,壬基酚与甲醛摩尔比1:1.5,反应温度85℃,反应时间4h。
2.研究不同因素对酯化产率的影响,确定了丙烯酸十八酯合成的最佳工艺,丙烯酸与十八醇摩尔比为1:1.5;对甲苯磺酸的质量分数为0.7wt%;对苯二酚的质量分数为0.4wt%;反应温度为120℃;反应时间为4h;携水剂按醇酸总质量的50%计。在此反应条件下,酯化产率可达93%以上。
3.以碳酸乙烯酯、1,3—丙烷磺内酯、马来酸酐、苯乙烯、丙烯酰胺、高级醇等为原料合成了酚醛树脂接枝碳酸乙烯酯(A)、酚醛树脂接枝1,3—丙烷磺内酯(B)、马来酸酐—丙烯酸十八酯二元共聚物(C)、马来酸酐—苯乙烯—丙烯酸十八酯三元共聚物(D)、马来酸酐—苯乙烯—丙烯酰胺酯化物(E)等五种梳型聚合物,分别考察了其对原油的降凝效果,发现A、B两种降凝剂降凝效果较差,仅为0～1℃。降凝剂E降凝效果最好,达到6.5℃。
4.研究了梳型聚合物的链段分布、亲油端链段、引发剂用量、聚合温度、聚合时间、降凝剂加入量、降凝剂处理温度等因素对原油降凝效果的影响。随着亲油链段的增长,降凝效果越来越好。随着引发剂加入量的增加,降凝效果越来越好,进一步增加,降凝效果开始变差。随着聚合温度的提高、聚合时间的延长,降凝效果越来越好,最后趋于稳定。
5.确定了C、D、E三种降凝剂的最佳合成工艺,马来酸酐:丙烯酸十八酯(mol)=1:3,引发剂用量0.5wt%,聚合温度105℃,聚合时间4h时,马来酸酐:苯乙烯:丙烯酸十八酯(mol)=2:1:6,引发剂用量0.7wt%,聚合温度100℃,聚合时间6h,马来酸酐:苯乙烯:丙烯酰胺(mol)=6:1:2,引发剂用量0.6wt%,聚合温度100℃,聚合时间7h。
In view of crude oils of Sudan 3/7 areas' character of high paraffin,high asphaltum,high solidification point and the mechanism of depressing pour point,a series of comb copolymer was synthesized and characterized by infrared(IR).Factors to influence pour point were also investigated.
The concrete content is as follows
1.Nonyl phenol and formaldehyde were used as a raw material to prepare linear polymer phenolics.Optimum technic conditions were obtained as follows:Zinc acetate as catalyst,PH= 4-7,T=85℃,t=4h,nonyl phenol versus formaldehyde =1:1.5(mol).
2.Factors to influence production rate of esterification were investigated.And optimum technic conditions were obtained as follows:acrylacid versus Octadecanol=1:1.5(mol);the content of toluene sulfonic acid is 0.7wt%;the content of hydroquinonequality is 0.4wt%;T=120℃;t= 4h.Under experimental conditions,the esterification production rate may reach above 93%.
3.A series of comb polymers was synthesized as follows:Phenolics-Ethylene carbonate graft copolymer(A),the Phenolicsstem—1,3-Propane sultone graft copolymer(B),Maleic anhydride -Octadecyl acrylate bipolymers(C),Maleic anhydride-Styrene-Octadecyl acrylate(D),Maleic anhydride-Styrene-Acrylamide ester(E).The efficiency of depressing pour point was also studied.Results showed that the efficiency of A,B to depress pour point was bad,only 0～1℃, E was the best,achieving 6.5℃.
4.The factors of comb polymer segment distribution,hydrophobic chain,the content of initiator, polymerization temperature,polymerization time,the content of PPD,and crude oil post-processing temperature to depress pour point were investigated.With the increases of hydrophobic chain,the efficiency of depressing pour point became better.With the increases of polymerization temperature and time,the efficiency of depressing pour point became better, finally tended to stable.
5.Optimum technics conditions for C,D and E were obtained as follows:Maleic anhydride: Octadecyl acrylate=1:3(mol),the content of initiator is 0.5wt%,T=105℃,t=4h for C;Maleic anhydride:Styrene:Octadecyl acrylate =2:1:6(mol),the content of initiator is 0.7wt%,T=100℃,t=6h for D;Maleic anhydride:Styrene:Acrylamide=6:1:2(mol),the content of initiator is 0.6wt%,T=100℃,t=8h.for E,repectively.
引文
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[2]Gamal.I.M.,Sabbagh.A.M.,Polymeric additives for improving the flow properties of wax distillate fuels and crudes,Fuel,1996,75(6):101-107
[3]张劲军,易黏高黏原油管输技术及其发展,中国工程科学,2002,4(6):89-93
[4]王彪,原油降凝剂的发展概况,精细石油化工,1985,6(5):43-47
[5]杜郢,原油热处理中加入降凝剂的研究,石油学报,1991,10(1):72-78
[6]Mieulet.P.,A new pour point depressant,World Oil,1966,5(10):95-101
[7]RodneyLee,A new synthesize of pour point depressant,US097953,2005-07-15
[8]Soni Hemant.R,Bharambe Dinakar.R,Synthesis and evaluation of polymeric additives as flow improvers for Indian crude oil,Ira.Poly.J.,2006,15(12):943-954
[9]Yu.T.Y.,Wang.J.L.,Jin.J.S.,Preparation of polymeric pour point depressants for shale oil,Energ.Sour.P.A-reco.Util.environ.Eff.,2006,28(8):757-762
[10]刘同春,原油降凝剂的开发与应用,化工进展,1991,15(4):12-15
[11]应圣康,共聚合反应,北京:化学工业出版社,1982,213-214
[12]林松,国内外化学降凝剂发展综述,油气集输,1992,(4):11-12
[13]郭意厚,石油工业进展,石油炼制,1991,22(6):26-32
[14]Garcia.M.C.,Carbogna.L.,Orea metal of petroleum,Sci.Eng.,2000,25(5):101-107
[15]刘菁,王复东,一种高凝原油的降凝剂,中国专利,1175614A,1998-10-15
[16]徐僖,夏长富,张洁辉等,乙烯一醋酸乙烯酯共聚物降凝作用的研究,油田化学,1984,10(2):232-241
[17]曹志强,马序忠,部分水解乙烯一醋酸乙烯酯共聚物防蜡降凝作用的研究,油田化学,1985,2(4):302-305
[18]Jorda.R.M.,Paraffin deposition and prevention in oil well,J.Pet.Tech.,1996,12(2):237-243
[19]Van Home.W.L.,Polymethacrylates as viscosity index improvers and pour point depressants,Ind.Eng.Chem.,1949,41(5):952-959
[20]陈建康,张建国,王燕舞,浅谈降凝剂的作用及应用现状,石油商技,2003,21(6):30-31
[21]Bern.R A.,Withers.V.R.,Cairns.J.R.,Wax deposition in crude oil pipelines,Euro.Petrol.Confer.,1990,28(10):206-211
[22]陈关喜,戚国荣,石明孝,乙烯-醋酸乙烯酯共聚物的合成表征及其降凝效果的研究,浙江大学学报,1994,28(3):338-348
[23]A.Willschke,D.Humbert,A.Rossi,Synthetic base stocks for low viscosity motor oils,J.Syn.Lubri.,1988,5(1):31-53
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